CN102268736B - Method for preparing silicon carbide nanowire array through gas phase interlayer diffusion reaction process - Google Patents
Method for preparing silicon carbide nanowire array through gas phase interlayer diffusion reaction process Download PDFInfo
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- CN102268736B CN102268736B CN 201110188615 CN201110188615A CN102268736B CN 102268736 B CN102268736 B CN 102268736B CN 201110188615 CN201110188615 CN 201110188615 CN 201110188615 A CN201110188615 A CN 201110188615A CN 102268736 B CN102268736 B CN 102268736B
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Abstract
The invention discloses a method for preparing a silicon carbide nanowire array through a gas phase interlayer diffusion reaction process. The method comprises the following steps of: fixing a porous substrate at a hole for communicating two channels of a two-channel quartz tube, and putting the two-channel quartz tube in a high temperature tube furnace; vacuumizing the two channels of the two-channel quartz tube by using a vacuum pump, and introducing argon; heating the high temperature tube furnace, introducing a carbon-containing precursor and a silicon-containing precursor into the two channels of the two-channel quartz tube respectively, protecting at the temperature, and cooling to room temperature, wherein the whole process is protected by introducing argon; and taking the substrate out of the two-channel quartz tube, ensuring that the surface of the substrate is coated by a layer of light blue semitransparent deposit with the thickness of more than 1cm, wherein the light blue semitransparent deposit is the prepared silicon carbide nanowire array. By adopting the gas phase interlayer diffusion reaction process, a highly ordered large-area silicon carbide nanowire array can be obtained easily and efficiently at low cost; and the silicon carbide nanowire array has good quality and low cost, and purification operation in the process of using nanowires is avoided.
Description
Technical field
The present invention relates to a kind of preparation method of conductor nano tube/linear array, particularly relate to a kind of gas phase inter-level diffusion reaction process preparation method of nanometer silicon carbide linear array.
Background technology
The nanometer silicon carbide linear array has important application prospect in fields such as the Study on Physical of one dimension Nano structure, the manufacturing of nano photoelectronic devices, the high-power nano-wire field effect transistor of temperature high performance high, Field Emission Display, advanced composite materials.
In recent years, many pieces of bibliographical informations the employing monocrystalline silicon piece as growth substrates and silicon source, take solid carbon material or carbonaceous gas as carbon source, prepare the method for nanometer silicon carbide linear array under hot conditions.For example, document " J.J.Niu, J.N.Wang, J.Phys.Chem.B, 2007,111,4368-4373 " discloses a kind of method for preparing the nanometer silicon carbide linear array take ZnS as catalyzer at monocrystalline silicon sheet surface.At first carbon powder particle is deposited on the boiler tube internal surface of High Temperature Furnaces Heating Apparatus, the monocrystalline silicon piece that then will be coated with the ZnS powder is placed on the boiler tube central position, prepares the nanometer silicon carbide linear array by chemical vapor deposition method at silicon chip surface at last.The method can obtain local order nanometer silicon carbide linear array preferably, but the monocrystalline silicon piece cost that the method adopts is higher, and the nano wire quality and the consistent appearance that obtain are relatively poor, the phenomenon that exists nano wire mutually to be wound around, these have a strong impact on nanometer silicon carbide linear array effect in every respect, and have increased process complexity and the operation easier in the application process.
Document " Y.J.Yang, G.W.Meng, X.Y.Liu, L.D.Zhang, Z.Hu, C.Y.He, Y.M.Hu, J.Phys.Chem.C, 2008,112:20126-20130 " discloses a kind of method that adopts the silicon nanowire array carborization to prepare the nanometer silicon carbide linear array.At first silicon chip is utilized hf etching to obtain the silicon nanowire array of high-sequential in reactor, then utilize ethanol with the silicon nanowire array carbonization under hot conditions, form the nanometer silicon carbide linear array.Although the method can obtain the nanometer silicon carbide linear array of high-sequential, but preparation process complex process, and the silicon carbide nanometer line that obtains is the polycrystalline structure of porous, and these will make the application of the aspects such as nanometer silicon carbide linear array nano photoelectronic devices, field-effect transistor, matrix material be restricted.
Document " Z.J.Li; J.L.Zhang; A.L.Meng, J.Z.Guo, Large-Area Highly-Oriented SiC Nanowire Arrays:Synthesis; Raman; and Photoluminescence Properties, J.Phys.Chem.B, 2006; 110,22382-22386 " discloses a kind of method for preparing the nanometer silicon carbide linear array take porous anodic aluminium oxide as template.The silicon monoxide gas that the method generates take silicon and silicon-dioxide mixed powder is as the silicon source, and propylene is carbon source, in the parallel nano pore internal reaction formation of deposits nanometer silicon carbide linear array of porous anodic alumina template.The method can obtain orderly nanometer silicon carbide linear array, but in preparation process, temperature and pressure is controlled complex process, and porous anodic alumina template fragility is large, cost is higher, and under hot conditions, alumina formwork crystal transition also may occur causes formwork structure to destroy.
The Chinese patent of document " application number is 200910160766.5 " discloses a kind of method of utilizing single-crystal silicon carbide sheet induced growth nanometer silicon carbide linear array.The method is take polymkeric substance such as polysilazanes as precursor, and the lattice by single-crystal silicon carbide sheet surface under hot conditions is induced the silicon carbide nanometer line oriented growth, the nanometer silicon carbide linear array that height of formation is orderly.The method can obtain orderly high quality nanometer silicon carbide linear array, but polymer raw material and single-crystal silicon carbide sheet cost that the method adopts are higher, the metal catalyst particles of introducing in preparation process needs the later stage to remove, and the Polymer-pyrolysis process also can produce the toxic gas of large amount of complex composition, serious threat staff's healthy and safe preparation process.
The Chinese patent of document " application number is 201010270528.2 " discloses a kind of method of utilizing dielectrophoresis technology oriented alignment silicon carbide nanometer line.At first the method adopts photoetching and lift-off technique produce electrode pair and apply ac voltage signal on silicon chip, then stable silicon carbide nanometer line solution is dripped between electrode pair, make nano wire realize oriented alignment under the effect of electric field force and moment.The method can make mixed and disorderly silicon carbide nanometer line align, and obtains the nanometer silicon carbide linear array, but the nano-wire array that the method obtains be only two-dimension plane structure, and appointed condition has relatively high expectations, the preparation process complexity, and operation easier is large.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the object of the present invention is to provide a kind of gas phase inter-level diffusion reaction process preparation method of nanometer silicon carbide linear array, safe, environmental friendliness, cost is low.
To achieve these goals, the technical solution used in the present invention is:
A kind of gas phase inter-level diffusion reaction process preparation method of nanometer silicon carbide linear array comprises the following steps:
The first step is fixed on two channels silica tube 2 with porous-substrates 1 and is communicated with in the perforate 5 of two passages, then two channels silica tube 2 is put into high temperature process furnances 3;
Second step vacuumizes 2 liang of passages of two channels silica tube with vacuum pump, when vacuum tightness reach-0.098MPa and stable after, then pass into argon gas to two channels silica tube 2 internal pressure 0.1MPa;
The 3rd step, switch on power, high temperature process furnances 3 temperature are risen to 1150 ℃-1300 ℃, two passages to two channels silica tube 2 pass into carbon containing precursor and siliceous precursor respectively, the flow range that passes into is 40-400sccm, and is incubated 0.5-2h at this temperature, then cools to room temperature, whole process is led to argon shield, and two channels silica tube 2 internal pressures remain on 0.1MPa;
The 4th step, take out substrate from two channels silica tube 2, substrate surface is covered by the light blue translucent settling that a layer height surpasses 1cm, and this light blue settling is the nanometer silicon carbide linear array that makes.
Wherein, described porous-substrates 1 is the porous material of ability temperature more than 1300 ℃, as: porous silicon carbide sheet, porous corundum sheet, porous silicon chip or porous stone ink sheet, the hole on porous-substrates 1 is communicating pores, its pore diameter range is 50nm-5mm.
Two channels silica tube 2 refers to that being parallel to channel-length direction in the passage of common silica tube has added quartzy dividing plate 4 and had channel structure, and perforate 5 is positioned on quartzy dividing plate 4, and being shaped as of perforate 5 is square or circular.
When the gaseous state precursor that described carbon containing precursor is the carbon containings such as carbon monoxide, methane, propylene, ethanol or 25 ℃, saturated vapor pressure is greater than the liquid precursor of 5.0KPa.
When described siliceous precursor is the siliceous gaseous state precursor such as silicon monoxide, silicon tetrachloride or 25 ℃, saturated vapor pressure is greater than the liquid precursor of 20.0KPa.
The invention has the beneficial effects as follows: owing to having adopted gas phase inter-level diffusion reaction process, can simply, efficiently and at low cost at multiple substrate surface, obtain the big area nanometer silicon carbide linear array of high-sequential, and quality be better.Technological process of the present invention does not need to adopt monocrystalline silicon piece, silicon carbide plate and silicon-containing polymer, and equipment used and operating procedure simple, thereby preparation cost is lower.Technological process of the present invention does not adopt metal catalyst, thereby the nanometer silicon carbide linear array purity of preparation is higher, has avoided the purification process in this nano wire use procedure.
Description of drawings
Fig. 1 is the structural representation of the two channels silica tube that adopts of the present invention, has arranged porous-substrates.
Fig. 2 is the structural representation of the two channels silica tube that adopts of the present invention, not yet arranges porous-substrates.
Fig. 3 is the stereoscan photograph of the nanometer silicon carbide linear array for preparing of the present invention.
Fig. 4 is the transmission electron microscope photo of the nanometer silicon carbide linear array for preparing of the present invention.
Fig. 5 is the X ray diffracting spectrum of the nanometer silicon carbide linear array for preparing of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further details.
Embodiment one
A kind of gas phase inter-level diffusion reaction process preparation method of nanometer silicon carbide linear array comprises the following steps:
The first step is fixed on two channels silica tube 2 with porous-substrates 1 and is communicated with in the perforate 5 of two passages, then two channels silica tube 2 is put into high temperature process furnances 3, and porous-substrates 1 is to be of a size of 60mm * 30mm * 1mm, and the aperture is the porous stone ink sheet of 2mm;
Second step vacuumizes 2 liang of passages of two channels silica tube with vacuum pump, when vacuum tightness reach-0.098MPa and stable after, then pass into argon gas to two channels silica tube 2 internal pressure 0.1MPa, to displace the air in silica tube;
The 3rd step, switch on power, heat-up rate with 7 ℃/min rises to 1150 ℃ with high temperature process furnances 3 temperature, then passes into CO (carbon monoxide converter) gas with the flow of 50sccm to a passage of two channels silica tube 2, take the high-purity argon gas of 70sccm flow as carrier gas, pass into silicon monoxide gas in another passage, be incubated 0.5h at this temperature, last powered-down cools to room temperature naturally, whole process is led to argon shield, and two channels silica tube 2 internal pressures remain on 0.1MPa;
The 4th step, take out substrate from two channels silica tube 2, substrate surface is covered by the light blue translucent settling that a layer height surpasses 1cm, and scanning electron microscope analysis shows: this light blue settling is the nanometer silicon carbide linear array of the high-sequential that makes.
Embodiment two
A kind of gas phase inter-level diffusion reaction process preparation method of nanometer silicon carbide linear array comprises the following steps:
The first step is fixed on two channels silica tube 2 with porous-substrates 1 and is communicated with in the perforate 5 of two passages, then two channels silica tube 2 is put into high temperature process furnances 3, and porous-substrates 1 is to be of a size of 60mm * 30mm * 1mm, and the aperture is the porous corundum sheet of 1mm;
Second step vacuumizes 2 liang of passages of two channels silica tube with vacuum pump, when vacuum tightness reach-0.098MPa and stable after, then pass into argon gas to two channels silica tube 2 internal pressure 0.1MPa, to displace the air in silica tube;
The 3rd step, switch on power, with the heat-up rate of 8 ℃/min, high temperature process furnances 3 temperature are risen to 1200 ℃, then take the argon gas of 80sccm flow as carrier gas, pass into the ethanol of gaseous state to a passage of two channels silica tube 2, take hydrogen as carrier gas, pass into the silicon tetrachloride of gaseous state in another passage, be incubated 1h at this temperature, last powered-down, naturally cool to room temperature, whole process is led to argon shield, and two channels silica tube 2 internal pressures remain on 0.1MPa;
The 4th step, take out substrate from two channels silica tube 2, substrate surface is covered by the light blue translucent settling that a layer height surpasses 0.8cm, and scanning electron microscope analysis shows: this light blue settling is the nanometer silicon carbide linear array of the high-sequential that makes.
Embodiment three
A kind of gas phase inter-level diffusion reaction process preparation method of nanometer silicon carbide linear array comprises the following steps:
The first step is fixed on two channels silica tube 2 with porous-substrates 1 and is communicated with in the perforate 5 of two passages, then two channels silica tube 2 is put into high temperature process furnances 3, and porous-substrates 1 is to be of a size of 60mm * 30mm * 1mm, and the aperture is the porous silicon chip of 80nm;
Second step vacuumizes 2 liang of passages of two channels silica tube with vacuum pump, when vacuum tightness reach-0.098MPa and stable after, then pass into argon gas to two channels silica tube 2 internal pressure 0.1MPa, to displace the air in silica tube;
The 3rd step, switch on power, heat-up rate with 9 ℃/min rises to 1250 ℃ with high temperature process furnances 3 temperature, then passes into methane with the 50sccm flow to a passage of two channels silica tube 2, and take the high-purity argon gas of 70sccm flow as carrier gas, pass into silicon monoxide gas in another passage, be incubated 1.5h at this temperature, last powered-down cools to room temperature naturally, whole process is led to argon shield, and two channels silica tube 2 internal pressures remain on 0.1MPa;
The 4th step, take out substrate from two channels silica tube 2, substrate surface is covered by the light blue translucent settling that a layer height surpasses 0.4cm, and scanning electron microscope analysis shows: this light blue settling is the nanometer silicon carbide linear array of the high-sequential that makes.
Embodiment four
A kind of gas phase inter-level diffusion reaction process preparation method of nanometer silicon carbide linear array comprises the following steps:
The first step is fixed on two channels silica tube 2 with porous-substrates 1 and is communicated with in the perforate 5 of two passages, then two channels silica tube 2 is put into high temperature process furnances 3, and porous-substrates 1 is to be of a size of 60mm * 30mm * 1mm, and the aperture is the porous silicon carbide sheet of 150 μ m;
Second step vacuumizes 2 liang of passages of two channels silica tube with vacuum pump, when vacuum tightness reach-0.098MPa and stable after, then pass into argon gas to two channels silica tube 2 internal pressure 0.1MPa, to displace the air in silica tube;
The 3rd step, switch on power, heat-up rate with 10 ℃/min rises to 1300 ℃ with high temperature process furnances 3 temperature, then passes into propylene with the 50sccm flow to a passage of two channels silica tube 2, and take hydrogen as carrier gas, pass into the silicon tetrachloride of gaseous state in another passage, be incubated 2h at this temperature, last powered-down cools to room temperature naturally, whole process is led to argon shield, and two channels silica tube 2 internal pressures remain on 0.1MPa;
The 4th step, take out substrate from two channels silica tube 2, substrate surface is covered by the light blue translucent settling that a layer height surpasses 0.6cm, and scanning electron microscope analysis shows: this light blue settling is the nanometer silicon carbide linear array of the high-sequential that makes.
As depicted in figs. 1 and 2, structural representation for two channels silica tube 2 of the present invention, two channels silica tube 2 refers to that being parallel to channel-length direction in the passage of common silica tube has added quartzy dividing plate 4 and had channel structure, perforate 5 is positioned on quartzy dividing plate 4, can be square or circular, porous-substrates 1 is fixed in perforate 5, and two input arrows in figure represent that respectively carbon containing precursor and siliceous precursor pass into two passages of two channels silica tube 2.
As shown in Figure 3, can find out that the order of the nanometer silicon carbide linear array that the present invention is prepared is better, be arranged parallel to each other between nano wire, the diameter uniformity only has a small amount of curling phenomenon.
As shown in Figure 4, can find out the prepared nanometer silicon carbide linear diameter of the present invention in the 50nm left and right, smooth surface is silicon oxide carbon coated SiClx nano cable structure.
As shown in Figure 5, the X-ray diffraction analysis result shows: the main component of the silicon carbide nanometer line that the present invention is prepared is β-SiC.Higher amorphous peak is that the amorphous silica layer by nanowire surface produces.
Above embodiment shows, the present invention adopts gas phase inter-level diffusion reaction process, prepared simply, efficiently and at low cost the nanometer silicon carbide linear array of high-sequential on the porous-substrates surface.This nanometer silicon carbide linear array can be applicable to Field Emission Display, nano-wire field effect transistor, nano photoelectronic devices, one dimension Nano structure Study on Physical, the fields such as advanced composite material.
The above is only one embodiment of the present invention, it not whole or unique embodiment, the conversion of any equivalence that those of ordinary skills take technical solution of the present invention by reading specification sheets of the present invention is claim of the present invention and contains.
Claims (9)
1. the gas phase inter-level diffusion reaction process preparation method of a nanometer silicon carbide linear array comprises the following steps:
The first step is fixed on porous-substrates (1) in the perforate (5) of two channels silica tube (2) connection two passages, then two channels silica tube (2) is put into high temperature process furnances (3);
Second step vacuumizes two channels silica tube (2) two passages with vacuum pump, when vacuum tightness reach-0.098MPa and stable after, then pass into argon gas to two channels silica tube (2) internal pressure 0.1MPa;
The 3rd step, switch on power, high temperature process furnances (3) temperature is risen to 1150 ℃ of-1300 ° of C, two passages to two channels silica tube (2) pass into carbon containing precursor and siliceous precursor respectively, the flow range that passes into is 40-400sccm, and is incubated 0.5-2h at this temperature, then cools to room temperature, whole process is led to argon shield, and two channels silica tube (2) internal pressure remains on 0.1MPa;
The 4th step, take out substrate from two channels silica tube (2), substrate surface is covered by the light blue translucent settling that a layer height surpasses 1cm, and this light blue settling is the nanometer silicon carbide linear array that makes.
2. the gas phase inter-level diffusion reaction process preparation method of nanometer silicon carbide linear array according to claim 1, is characterized in that, described porous-substrates (1) is the porous material of ability temperature more than 1300 ℃.
3. the gas phase inter-level diffusion reaction process preparation method of nanometer silicon carbide linear array according to claim 1 and 2, is characterized in that, described porous-substrates (1) is porous silicon carbide sheet, porous corundum sheet, porous silicon chip or porous stone ink sheet.
4. the gas phase inter-level diffusion reaction process preparation method of nanometer silicon carbide linear array according to claim 1 and 2, is characterized in that, the hole on described porous-substrates (1) is communicating pores, and its pore diameter range is 50nm-5mm.
5. the gas phase inter-level diffusion reaction process preparation method of nanometer silicon carbide linear array according to claim 1, it is characterized in that, described two channels silica tube (2) refers to that being parallel to channel-length direction in the passage of common silica tube has added quartzy dividing plate (4) and had channel structure.
6. the gas phase inter-level diffusion reaction process preparation method of nanometer silicon carbide linear array according to claim 5, is characterized in that, described perforate (5) is positioned on quartzy dividing plate (4).
7. the gas phase inter-level diffusion reaction process preparation method of nanometer silicon carbide linear array according to claim 1, is characterized in that, described perforate (5) is square or circular.
8. the gas phase inter-level diffusion reaction process preparation method of nanometer silicon carbide linear array according to claim 1, is characterized in that, described carbon containing precursor is carbon monoxide, methane, propylene or ethanol.
9. the gas phase inter-level diffusion reaction process preparation method of nanometer silicon carbide linear array according to claim 1, is characterized in that, described siliceous precursor is silicon monoxide or silicon tetrachloride.
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| CN105133017B (en) * | 2015-07-08 | 2016-11-02 | 宁波工程学院 | The method of regulation and control SiC nano-array density |
| CN106587002A (en) * | 2016-11-23 | 2017-04-26 | 东莞劲胜精密组件股份有限公司 | Preparation method for carbon micro-tube |
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